ASTM-D7597 Standard Test Method for Determination of Diisopropyl Methylphosphonate, Ethyl Hydrogen Dimethylamidophosphate, Ethyl Methylphosphonic Acid, Isopropyl Methylphosphonic Acid, Methylphosphonic Acid and Pinacolyl Methylphosphonic Acid in Water by Liquid Chromatography/Tandem Mass Spectrometry

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Standard Test Method for Determination of Diisopropyl Methylphosphonate, Ethyl Hydrogen Dimethylamidophosphate, Ethyl Methylphosphonic Acid, Isopropyl Methylphosphonic Acid, Methylphosphonic Acid and Pinacolyl Methylphosphonic Acid in Water by Liquid Chromatography/Tandem Mass Spectrometry
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Scope

1.1 This procedure covers the determination of diisopropyl methylphosphonate (DIMP), ethyl hydrogen dimethylamidophosphate (EHDMAP), ethyl methylphosphonic acid (EMPA), isopropyl methylphosphonic acid (IMPA), methylphosphonic acid (MPA) and pinacolyl methylphosphonic acid (PMPA) (referred to collectively as organophosphonates in this test method) in surface water by direct injection using liquid chromatography (LC) and detected with tandem mass spectrometry (MS/MS) using electrospray ionization (ESI). These analytes are qualitatively and quantitatively determined by this test method. This test method adheres to single reaction monitoring (SRM) mass spectrometry.

1.2 This test method has been developed by U.S. EPA Region 5 Chicago Regional Laboratory (CRL).

1.3 The values stated in SI units are to be regarded as standard. No other units of measurement are included in this standard.

1.4 The detection verification level (DVL) and reporting range for the organophosphonates are listed in Table 1.

TABLE 1 Detection Verification Level and Reporting Range

Analyte

ESI Mode

DVL (μg/L)

Reporting Range (μg/L)

Diisopropyl methylphosphonate

Positive

1

5–150

Ethyl hydrogen dimethylamidophosphate

Negative

0.25

5–150

Ethyl hydrogen dimethylamidophosphate

Positive

0.25

5–150

Ethyl methylphosphonic acid

Negative

5

50–1500

Ethyl methylphosphonic acid

Positive

5

50–1500

Isopropyl methylphosphonic acid

Negative

10

50–1500

Isopropyl Methylphosphonic acid

Positive

5

50–1500

Methylphosphonic acid

Negative

20

100–1500

Methylphosphonic acid

Positive

10

50–1500

Pinacolyl methylphosphonic acid

Negative

5

50–1500

Pinacolyl methylphosphonic acid

Positive

5

50–1500

1.4.1 The DVL is required to be at a concentration at least three times below the reporting limit (RL) and have a signal/noise ratio greater than 3:1. Fig. 1 displays the signal/noise ratios at the DVLs for the organophosphonates in the ESI positive mode and Fig. 2 in the ESI negative mode.

FIG. 1 Example ESI Positive Mode SRM Chromatograms Signal/Noise Ratios

Example ESI Positive Mode SRM Chromatograms Signal/Noise
 RatiosExample ESI Positive Mode SRM Chromatograms Signal/Noise
 Ratios

FIG. 2 Example ESI Negative Mode SRM Chromatograms Signal/Noise Ratios

Example ESI Negative Mode SRM Chromatograms Signal/Noise
 RatiosExample ESI Negative Mode SRM Chromatograms Signal/Noise
 Ratios

1.4.2 The reporting limit is the concentration of the Level 1 calibration standard as shown in Table 2 for the organophosphonates except for MPA in the ESI negative mode which is at Level 2 due to not meeting the DVL criteria at the lower concentration level. The DVL for MPA in the ESI negative mode is at 20 μg/L, which forces a raised reporting limit. However, the multi-laboratory validation required a spike of all target analytes at Level 1 concentrations. The mean recovery for MPA in the ESI negative mode at this level was 98.7 % as shown in Table 3. If your instrument’s sensitivity can meet the requirements in this test method, MPA may have a 50 μg/L reporting limit.

TABLE 2 Concentrations of Calibration Standards (PPB)

Analyte/Surrogate

LV 1

LV 2

LV 3

LV 4

LV 5

LV 6

LV 7

Diisopropyl methylphosphonate

5

10

20

35

50

100

150

Ethyl hydrogen dimethylamidophosphate

5

10

20

35

50

100

150

Ethyl methylphosphonic acid

50

100

200

350

500

1000

1500

Isopropyl methylphosphonic acid

50

100

200

350

500

1000

1500

Methylphosphonic acid

50

100

200

350

500

1000

1500

Pinacolyl methylphosphonic acid

50

100

200

350

500

1000

1500

DIMP-D14 (Surrogate)

5

10

20

35

50

100

150

PMPA-13C4 (Surrogate)

25

50

100

175

250

500

750

MPA-D3 (Surrogate)

25

50

100

175

250

500

750

TABLE 3 Multi-Laboratory Recovery Data in Reagent Water

Analyte

ESI
Mode

Spike Conc.
(ppb)

# Results

# Labs

Bias

Precision

Mean
Recovery
(%)

Min
Recovery
(%)

Max
Recovery
(%)

Overall SD
(%)

Pooled
within-lab
SD (%)

Overall
RSD (%)

Pooled
within-lab
RSD (%)

DIMP

Pos

5

16

4

95.1

65.8

136.0

17.6

19.4

21.3

22.4

DIMP

Pos

10

19

5

98.2

80.0

121.0

6.1

5.5

13.6

13.8

DIMP

Pos

25

26

6

102.9

74.4

128.0

5.6

5.7

14.5

14.1

DIMP

Pos

125

22

5

96.6

80.4

120.0

4.4

4.5

11.0

11.4

DIMP-D14

Pos

25

86

6

102.6

54.8

127.6

9.8

9.5

11.2

10.9

EHDMAP

Neg

5

12

3

57.5

0.0

220.0

31.4

22.3

71.1

123.6

EHDMAP

Neg

10

16

4

47.1

0.0

178.0

13.3

10.8

66.8

142.0

EHDMAP

Neg

25

22

5

84.1

54.0

141.2

6.9

6.6

22.9

27.3

EHDMAP

Neg

125

18

4

87.4

64.2

141.6

5.0

5.1

25.4

29.1

EHDMAP

Pos

5

16

4

77.0

0.0

134.2

7.4

8.0

51.4

66.8

EHDMAP

Pos

10

20

5

70.0

0.0

143.0

7.7

10.0

53.6

76.5

EHDMAP

Pos

25

26

6

89.6

60.0

128.8

5.2

6.2

23.5

26.2

EHDMAP

Pos

125

22

5

87.5

59.0

123.2

5.2

6.0

23.9

27.3

EMPA

Neg

50

16

4

110.1

74.8

170.6

22.4

17.2

25.6

23.3

EMPA

Neg

100

20

5

108.3

87.7

175.0

11.1

8.7

24.8

22.9

EMPA

Neg

250

26

6

104.8

82.0

122.6

6.1

5.5

11.8

11.3

EMPA

Neg

1250

22

5

101.5

87.2

126.4

8.4

8.1

11.2

11.0

EMPA

Pos

50

16

4

95.4

77.6

122.8

12.9

13.3

13.1

13.7

EMPA

Pos

100

20

5

96.0

61.4

132.5

9.5

9.5

15.9

16.6

EMPA

Pos

250

26

6

99.7

70.0

133.2

5.9

5.4

18.2

18.2

EMPA

Pos

1250

21

5

93.9

84.0

108.4

2.7

3.0

7.7

8.2

IMPA

Neg

50

16

4

88.0

56.6

140.4

23.7

26.0

23.5

26.7

IMPA

Neg

100

20

5

88.0

68.5

118.0

12.9

14.3

13.4

15.2

IMPA

Neg

250

26

6

98.1

72.8

144.0

13.1

11.9

19.2

19.6

IMPA

Neg

1250

21

5

90.7

73.1

103.0

5.5

6.1

8.7

9.6

IMPA

Pos

50

16

4

98.3

47.8

139.6

19.2

20.5

27.2

27.7

IMPA

Pos

100

19

5

95.4

72.3

120.5

9.8

10.3

12.4

13.0

IMPA

Pos

250

26

6

97.0

79.2

188.4

7.4

7.6

10.9

11.2

IMPA

Pos

1250

21

5

91.3

70.4

115.5

5.1

5.2

11.4

12.5

MPA

Neg

50

16

4

98.7

3.3

175.0

14.2

25.3

60.5

61.3

MPA

Neg

100

20

5

100.0

41.9

142.0

8.9

9.2

30.8

30.8

MPA

Neg

250

26

6

99.5

66.0

124.5

7.6

7.6

14.5

14.5

MPA

Neg

1250

22

5

102.7

81.8

130.5

10.5

9.9

12.4

12.1

MPA

Pos

50

16

4

68.3

9.8

139.6

13.4

20.3

36.6

53.6

MPA

Pos

100

20

5

80.5

48.4

149.7

14.0

12.6

26.8

33.3

MPA

Pos

250

26

6

91.7

33.9

153.7

8.0

7.8

31.8

34.7

MPA

Pos

1250

22

5

95.8

31.8

208.2

12.6

8.3

43.4

45.3

MPA-D3

Neg

250

84

6

111.2

57.2

190.8

16.2

12.5

30.0

26.9

MPA-D3

Pos

250

68

5

104.4

58.4

151.8

14.3

14.0

18.0

17.3

PMPA

Neg

50

15

4

87.8

77.6

124.4

8.4

8.2

13.8

15.7

PMPA

Neg

100

19

5

91.6

83.6

98.2

2.8

3.0

4.4

4.8

PMPA

Neg

250

26

6

101.0

77.2

123.8

5.0

4.8

12.1

12.0

PMPA

Neg

1250

22

5

99.2

84.8

126.5

4.9

4.8

12.3

12.4

PMPA

Pos

50

16

4

90.8

60.8

148.8

15.8

16.1

25.6

28.2

PMPA

Pos

100

15

4

95.2

86.8

114.0

3.8

4.0

7.9

8.3

PMPA

Pos

250

20

5

103.8

85.2

136.1

4.5

3.8

15.3

14.7

PMPA

Pos

1250

12

3

99.8

88.8

117.5

5.2

5.0

7.5

7.5

PMPA-13C6

Neg

250

83

6

99.5

74.8

128.3

9.4

9.2

11.1

11.1

1.5 This standard does not purport to address all of the safety concerns, if any, associated with its use. It is the responsibility of the user of this standard to establish appropriate safety and health practices and determine the applicability of regulatory limitations prior to use.

1.6 This international standard was developed in accordance with internationally recognized principles on standardization established in the Decision on Principles for the Development of International Standards, Guides and Recommendations issued by the World Trade Organization Technical Barriers to Trade (TBT) Committee.

Keywords

liquid chromatography; mass spectrometry; organophosphonates;; ICS Number Code 13.060.50 (Examination of water for chemical substances)

To find similar documents by ASTM Volume:

11.02 (Water (II))

To find similar documents by classification:

13.060.50 (Examination of water for chemical substances)

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Document Number

ASTM-D7597-16(2017)

Revision Level

2016 R17 EDITION

Status

Current

Modification Type

Reapproval

Publication Date

July 15, 2017

Document Type

Test Method

Page Count

13 pages

Committee Number

D19.06